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In recent years, researchers have devoted considerable effort to the study of high crystalline titanium‐oxo clusters (TOCs), because TOCs are considered to be the molecular analogs of TiO2 nanoparticles and have the potential to be utilized as effective cleaning and catalytic materials. Two new tartrate‐anchored tetranuclear TOCs functionalized with chromophore ligand of p‐nitrobenzoate (NB)/p‐toluenesulfonate (TS), namely, [Ti4(TA)(NB)2(OiPr)10] (1, H4TA = tartaric acid) and [Ti4(TA)(TS)2(OiPr)10] (2), were synthesized and their structures were characterized by various methods. The molecular structure analyses indicated that 1 and 2 are all tetranuclear {Ti4} TOCs, in which tartrate appears as a hexadentate μ4‐bridging ligand while p‐nitrobenzoate/p‐toluenesulfonate acts as a bidentate μ2‐bridging ligand. TOCs 1 and 2 are of good thermal and solvent stability. Furthermore, their photocurrent responses and photocatalytic degradation activities towards methylene blue (MB) were also investigated. In the presence of H2O2, the photocatalytic degradation efficiencies of MB by 1 and 2 are about 84.43% and 71.00%, respectively, at room temperature under visible light irradiation for 60 min. These findings shed light on designing efficient polycarboxylate‐based TOCs photocatalysts. [ABSTRACT FROM AUTHOR]